You are on page 1of 48

Experiment 7

Post-Lab Discussion

Quantitative Determination of Total


Hardness in Drinking Water by
Complexometric EDTA Titration

26 March 2019 | Chem 26.1


Mervin John C. Manguera, RCh | Institute of Chemistry, UP-Diliman
EXPERIMENT 7 POST-LAB DISCUSSION

COORDINATION CHEMISTRY
- the study of the formation of
coordination compounds or
complexes, often accompanied by
color change

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

COORDINATION COMPOUNDS
- composed of a metal atom or ion
(coordination center) and anions with
one or more unshared electrons
(ligand)

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

COORDINATION COMPOUNDS
- Lewis acid and base interaction
- held only by electrostatic interaction

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

CRYSTAL FIELD THEORY

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Solutions containing [M(H2O)6]n+ ions with


M = Sc3+, Cr3+, Co2+, Ni2+, Cu2+ and Zn2+.

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Other factors affecting Δ


1. Oxidation state of metal center
2. d-orbitals involved
3. Number and geometry of ligands

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Water
Polymer
quality
industry
assessment

Ink industry Electroplating

Applications of
Coordination
compounds

Photography Mineralogy

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

COMPLEXOMETRIC TITRATION
- a type of titration based on complex
formation between the analyte and
titrant
- useful in the determination of
[Mn+] in the solution

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Conditions for
Complexometric Titration
1. The reaction reaches equilibrium
rapidly as each portion of titrant is
added.

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Conditions for
Complexometric Titration
2. Interfering situations do not arise.
No other complex formed other than
that with the analyte

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Conditions for
Complexometric Titration
3. A complexometric indicator is
available.

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

EDTA
- a tetraprotic acid (H4Y)
- a hexadentate ligand
- used in complexometric titrations
- forms stable 1:1 complex with
many metals

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

METALLOCHROMIC INDICATORS
- organic dyes that form a colored
complex with metal ions that is
distinguishable from the free indicator
color

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

xylenol orange for gallium,


indium and scandium titration

eriochrome black T for calcium,


magnesium and aluminum
titration

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

WATER HARDNESS
- measure of total ions present in
water
- predominant ions: Ca2+ and Mg2+

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Mg + HIn
2+ 2-
→ MgIn + H - +

Ca + HIn
2+ 2-
→ CaIn + H - +

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

MgIn + Y + H
- 4- +
→ MgY 2-
+ HIn 2-

CaIn- + Y4- + H+ → CaY 2-


+ HIn2-

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

pH dependence of titration
- in very low pH (< 3.0): H4Y
- at pH 3.0 – 10.0: H3Y & H2Y
- 2-

- at pH > 10.0: Y4-

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

At low pH, [H+] is high, so the


backward reaction is favored.

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Minimum pH for effective


titrations of various metal
ions with EDTA.

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

RESULTS AND DISCUSSION

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

MASKING
- removal of interferences in an
analysis by formation of precipitates
or stable complexes

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

MASKING AGENTS
- CN-: Cd, Zn, Hg, Cu, Co, Ni, Ag, Pt
- CN- + ascorbic acid: Fe
- Triethanolamine: Ti(IV), Fe(III), Al
- I : Hg
-

- NH4F: Al, Fe(III), Ti(IV), Sn(II)


- high pH (> 10.0): Mg
QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING
WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
1. What is water hardness and what
is the relevance of quantifying it?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
2. What are the advantages and
disadvantages of hard water?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
3. How does complexometric titration
work? What are the advantages of
complexometric titration?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
4. Why was EDTA employed as a
complexation agent in the
experiment?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
5. Why is eriochrome black T
necessary in the quantitation? How
does it indicate the complete reaction
of the analytes?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
6. Why were MgCl2·6H2O added in
the preparation of EDTA solution?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
7. Why is the addition of NaOH
allowed, but not really necessary in
the preparation of the EDTA titrant?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
8. Why was HCl added in the
preparation of CaCO3 solution?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
9. What is the importance of
maintaining the pH = 10 and
choosing NH3-NH4Cl as the buffer?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
10. What are the possible sources of
errors and their effects on the
calculated parameters? Rationalize.

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019
EXPERIMENT 7 POST-LAB DISCUSSION

Guide questions:
11. What improvements can be made
on the experimental design, probably
to be more specific on the analyte
titrated?

QUANTITATIVE DETERMINATION OF TOTAL HARDNESS IN DRINKING


WATER BY COMPLEXOMETRIC EDTA TITRATION | 26 March 2019

You might also like